CN108588428B - The electrochemical method of arsenic and alkali in a kind of separation arsenic alkaline slag - Google Patents
The electrochemical method of arsenic and alkali in a kind of separation arsenic alkaline slag Download PDFInfo
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- CN108588428B CN108588428B CN201810486539.0A CN201810486539A CN108588428B CN 108588428 B CN108588428 B CN 108588428B CN 201810486539 A CN201810486539 A CN 201810486539A CN 108588428 B CN108588428 B CN 108588428B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses the electrochemical methods of arsenic and alkali in a kind of separation arsenic alkaline slag, and this method is that arsenic alkaline slag is carried out oxidation water logging, obtains the leaching liquor of arsenic-containing alkaline dregs of containing sodium carbonate and natrium arsenicum；It is cathode by electrolyte, ferroelectricity extremely anode and carbon electrode of sodium carbonate liquor, is electrolysed, generates active ferrous hydroxide in the electrolytic solution；Leaching liquor of arsenic-containing alkaline dregs is added into the electrolyte containing active ferrous hydroxide, is electrolysed, ferric arsenate crystal settling is generated.This method passes through oxidation water logging, realize the separation of arsenic alkaline slag antimony, arsenic in leachate is converted to the arsenic acid iron particle of good crystallinity by electrochemical method again, realize efficiently separating for arsenic and alkali, this method energy is quick, goes arsenic removal from strong alkali solution efficiently at low cost, reduce the use of oxidant in arsenic removal process, the operation is simple and convenient for this method, meets industrialized production.
Description
Technical field
The present invention relates to a kind of processing methods of arsenic alkaline slag, in particular to a kind of to be realized in arsenic alkaline slag using electrochemical method
The efficient separation method of arsenic and alkali, belongs to technical field of resource comprehensive utilization.
Background technique
In naturally occurring antimony ore be associated with arsenic minerals, wherein mispickel (FeAsS) is that arsenic is primarily present form more.In
During pyrometallurgical smelting, most arsenic can be oxidized volatilization in antimony ore, and remaining part enters in reduction furnace, and thus output is thick
Antimony.The principle for industrially often utilizing its (high oxide of arsenic and antimony) thermodynamic tendency difference, using pyro-refining by arsenic
Preferential oxidation can finally obtain the arsenic alkaline slag containing arsenic about 5%~10%, and have reached the antimony ore of arsenic content removal standard.
China is traditional antimony producing country, and antimonial resources country the most abundant, antimony product specie and yield are equal in the world
It occupies first place in the world.China's antimony smelts the area most concentrated in the tin ore Mountain area of Lengshuijiang, Hunan, this area's antimonial resources
Reserves account for 60% or more of world's gross reserves, and antimony product yield accounts for the 80% of world's total amount, and therefore, which is known as the world ＂ antimony
All ＂.Currently, most in the antimony smelting enterprise in China use pyrometallurgy, account for about overall 95%.The metallurgical production of antimony is not
Pipe is all to generate arsenic alkaline slag using pyrometallurgy or using hydrometallurgy.
Arsenic and antimony in arsenic alkaline slag all have carcinogenic effect, are classified as and pay the utmost attention to by the World Health Organization, the U.S., European Union etc.
Pollutant.Processing for kind of alkaline residue is all the antimony smelting industry most thorny issue all the time, has become global difficulty
Topic.Arsenic alkaline slag is dealt with improperly once revealing, and will penetrate into Soil Surrounding, underground water and neighbouring rivers and lakes are to ecological environment
Serious pollution is caused, more seriously, arsenic can be absorbed by the human body by water source and food chain, seriously endanger human body
Health, in some instances it may even be possible to will lead to death.
Not only contain the metallic antimony that can be recycled in view of arsenic alkaline slag, but also have the characteristic of hypertoxic natrium arsenicum, makes it very
It is difficult directly to carry out secondary smelting, it cannot directly abandon.Therefore, being handled arsenic alkaline slag and being recycled seems necessary.
Pyrometallurgical smelting is that the arsenic in arsenic alkaline slag is oxidized to As by way of oxidizing roasting2O3, or refining or anti-dazzled by blast furnace
It penetrates furnace and irons refining method, by thick As2O3Reduction refining is to be made elemental arsenic.As is produced using oxidizing roasting volatility process processing arsenic alkaline slag2O3
Secondary pollution is easily brought, and it is ineffective to handle the lower arsenic alkaline slag containing arsenic.Using hydrometallurgy method processing arsenic alkaline slag its
Main principle is that water can be dissolved in using arsenic in arsenic alkaline slag, and the property that antimonic salt is not soluble in water will be crushed to certain particle size
Arsenic alkaline slag realizes the separation of antimony and arsenic using the method leached well.The major defect of calcium salt precipitation method is still first
Produce toxic arsenic calcium slag, and arsenic calcium slag do not allow also it is easy to handle: secondly calcium salt method depletion of spirit effect is not highly desirable, calcium salt
Concentration needs are much excessive, can just arsenic content be made to be reduced to reduced levels, this needs to consume very more calcium salts, not from basic
The upper threat for solving arsenic pollution.Molysite deposition limited resource is numerous, it is difficult to the iron hydroxide of filtering, it is difficult to the arsenic scum of processing,
Adsorption coprecipitation reaction influenced by each factor etc., all at its widely applied limiting factor.
Summary of the invention
For high-alkali arsenic slag in the prior art processing method there are low efficiency, arsenic alkali separation be not thorough, in separation process
It consumes energy the defects of big, the purpose of the invention is to provide one kind to pass through electrolytic method next life Viability ferrous hydroxide and hydrogen-oxygen
Change ferrous iron, and the method for generating stable, good crystallinity precipitated ferric arsenate using iron hydroxide absorption and conversion arsenic acid radical ion,
The method achieve quick, the efficient removals of arsenic in strong basicity leaching liquor of arsenic-containing alkaline dregs, and the operation is simple and convenient, and low energy consumption,
The use that oxidant in electric flocculation arsenic removal process can be reduced, meets industrialized production.
In order to achieve the above technical purposes, the present invention provides it is a kind of separation arsenic alkaline slag in arsenic and alkali electrochemical method,
Itself the following steps are included:
1) arsenic alkaline slag is subjected to Oxidation Leaching, obtains the leaching liquor of arsenic-containing alkaline dregs of containing sodium carbonate and natrium arsenicum；
2) sodium carbonate liquor using concentration less than 20g/L is cathode as electrolyte, ferroelectricity extremely anode and carbon electrode, is carried out
Electrolysis generates active ferrous hydroxide in the electrolytic solution；
3) 1) gained leaching liquor of arsenic-containing alkaline dregs in is added into the electrolyte containing active ferrous hydroxide in 2), carries out electricity
Solution generates ferric arsenate crystal settling.
Technical solution of the present invention key is to realize that natrium arsenicum is converted in leaching liquor of arsenic-containing alkaline dregs by electrolytic method
Stablize, the precipitated ferric arsenate of good crystallinity, to be easily achieved the separation of arsenic and alkali.With weakly alkaline carbon in electrolytic process
Acid sodium solution is as electrolyte, and with ferroelectricity extremely anode, and inertia carbon electrode is cathode, electrolysis a period of time is first carried out, from iron
Part Fe is discharged in electrode2+Ion, this part Fe2+Ion forms active ferrous hydroxide under weak basic condition.Active hydrogen-oxygen
Change iron to play an important role in subsequent leaching liquor of arsenic-containing alkaline dregs electrolytic process, active ferrous iron can be generated with inductive anode area
Cation generates ferrous hydroxide polymer, while anode OH-O is precipitated in oxidation2, ferrous hydroxide polymer is oxidized to hydroxide
Iron colloid, arsenate ionic adsorption is on iron hydroxide surface and generates ferric arsenate, and ageing, crystallization, growth, precipitating gradually occurs,
The preferable bulky grain precipitated ferric arsenate of crystallinity is formed, ferric arsenate and lye separative efficiency are greatly improved.
Technical solution of the present invention electrolytic process is divided into the progress of two steps, and the first step is mainly the weak basic condition in low concentration
Lower electrolytic preparation ferrous hydroxide presoma, and hydroxyl oxygen can occur for anode ferroelectricity polar region under the strong alkaline condition of high concentration
Change reaction, the electrolysis of iron electrode is difficult to occur, therefore the purpose of this step essentially consists in the active ferrous hydroxide presoma of preparation；
Second one-step electrolysis: under the induction of presoma, the electrolysis of iron electrode and it is hydroxy oxidation simultaneously occur, ferrous hydroxide aoxidize
It is reacted for high activity iron hydroxide with arsenate.
Preferred scheme, by arsenic alkaline slag and oxidant by ore grinding and plus water logging go out, be separated by solid-liquid separation, obtain containing sodium carbonate and
The leaching liquor of arsenic-containing alkaline dregs of natrium arsenicum.The Oxidation Leaching of arsenic alkaline slag is mainly that the arsenic in arsenic alkaline slag is oxidized to readily soluble form to soak
Out, and antimony is oxidized to insoluble matter form, to realize the separation of antimony.
Preferred scheme, the arsenic alkaline slag and oxidant ore grinding to granularity meet -200 mesh granular mass degrees and account for
80% or more.By ore grinding to appropriate granularity, is conducive to the oxidizing reaction rate for improving leaching process, improves leaching efficiency.
Preferred scheme, the oxidant are sodium peroxide, and the relative usage of the oxidant is by arsenous in arsenic alkaline slag
1~1.2 times of oxidant theoretical molar amount needed for hydrochlorate and antimonite are oxidized to arsenate and stibate.
Preferred scheme, the Oxidation Leaching condition are as follows: liquid-solid ratio L/S be 3~6mL/1g, stirring rate be 80~
100r/min, extraction temperature are 80~85 DEG C, 0.5~1.5h of extraction time.By Oxidation Leaching, so that arsenic and alkali in arsenic alkaline slag
Into solution, and antimony exists in the form of insoluble matter, realizes the separation of antimony.
Preferred scheme, 2) electrolytic condition in are as follows: the mass percent concentration of sodium carbonate is 0.5~1% in electrolyte,
Electrolyte temperature is 50~60 DEG C, and current density is 20~40mA/cm2, electrolysis time is 20~40min.
Preferred scheme, 3) electrolytic condition in are as follows: electrolyte temperature is 50~60 DEG C, and current density is 10~30mA/
cm2, electrolysis time is 1h~1.5h.
Recycling can be realized by being simply separated by filtration in precipitated ferric arsenate of the invention, and the ferric arsenate arsenic slag of recycling passes through
Pyrogenic attack is changed into As2O5Or simple substance As, resource utilization can be carried out, filtrate is sodium carbonate liquor, after crystallized processing
Return to antimony smelting system.
The electrochemical method that arsenic is separated with alkali in a kind of arsenic alkaline slag of the invention, comprising the following specific steps
Step 1: the Oxidation Leaching of arsenic in arsenic alkaline slag
A certain amount of arsenic alkaline slag is taken, solid oxidizer sodium peroxide is added, 10~15min of ore grinding guarantees that -200 mesh account for 80%
More than, a certain amount of water is added, liquid-solid ratio L/S is about 3~6mL/g, stirs 80~100r/min, 80~85 DEG C of extraction temperature, soaks
Time 1h or so out, filtering gained filtrate are the mixed solution of containing sodium carbonate and natrium arsenicum, and leached mud returns to antimony smelting system.
Step 2: the preparation of ferrous hydroxide presoma
The solution that sodium carbonate is made into 1% is poured into electrolytic cell, anode is iron electrode, and cathode is that carbon electrode is electrolysed
30min, current density 30mA/cm2, reaction temperature is 50~60 DEG C, iron electrode Fe2+Ion releasing and under weak basic condition
Form ferrous hydroxide polymer presoma.
Step 3: leaching liquor of arsenic-containing alkaline dregs electrolytic oxidation
Leaching liquor of arsenic-containing alkaline dregs is added in electrolytic cell, using iron-based electrode as anode, using carbon resistance rod as cathode, is electrolysed,
Active ferrous iron cation is generated in anode region, under the induction of ferrous hydroxide presoma, is precipitated and to generate ferrous hydroxide more
Aggressiveness, while anode OH-O is precipitated in oxidation2, ferrous hydroxide polymer is oxidized to ferric hydroxide colloid, and arsenate ionic adsorption exists
Iron hydroxide surface simultaneously generates ferric arsenate, and ageing, crystallization, growth, precipitating gradually occurs, forms the preferable bulky grain arsenic of crystallinity
Sour iron precipitating, greatly improves arsenic and lye separative efficiency；Gained arsenic slag is changed into As through pyrogenic attack2O5Or simple substance As is carried out
Resource utilization, filtrate are sodium carbonate liquor, and antimony smelting system is returned after crystallized processing.
Compared with the prior art, technical solution of the present invention bring advantageous effects:
1, technical solution of the present invention first passage electrochemical method to realize, divide in leaching liquor of arsenic-containing alkaline dregs by arsenic and the efficient of alkali
From, there is the separation of arsenic alkali thoroughly, low energy consumption, at low cost, it is without secondary pollution the advantages that, relatively existing pyrometallurgical smelting, without secondary
Pollution, separating effect is more preferable, and relatively existing wet-treating process, reduces the use cost of a large amount of calcium salts, reduces arsenic
Recovery difficult.
2, the electrochemical method that arsenic is separated with alkali in arsenic alkaline slag of the invention uses ferroelectricity extremely anode, alkalescent sodium carbonate
Solution is electrolyte, first prepares active ferrous hydroxide, recycles the inducing action of ferrous hydroxide to be precipitated and generates hydroxide
Ferrous polymer, then aoxidized by Oxygen anodic evolution, ferrous hydroxide polymer is oxidized to ferric hydroxide colloid, arsenic acid radical ion
It is adsorbed on ferric hydroxide colloid surface and generates ferric arsenate, ageing, crystallization, growth, precipitating gradually occurs, it is preferable to form crystallinity
Bulky grain precipitated ferric arsenate, separation can be realized by being simply separated by filtration, so that greatly improving arsenic separates effect with lye
Rate, relatively existing molysite deposition method, substantially increases the separating effect of arsenic scum.
3, the electrochemical method that arsenic is separated with alkali in arsenic alkaline slag of the invention, it is easy to operate, reduce electric flocculation arsenic removal process
The use of middle oxidant, cost and low energy consumption meet industrialized production.
Detailed description of the invention
[Fig. 1] is electrolysis unit schematic diagram of the invention；
[Fig. 2] is process flow diagram of the invention.
Specific embodiment
Following embodiment is intended to further illustrate the content of present invention, rather than limits the protection model of claim of the invention
It encloses.
Embodiment 1
The secondary arsenic alkaline slag in Hunan antimony smeltery is handled using this process, As content is up to 4.8%, Sb content
5.42%, carbonate content 25.31%.50g arsenic alkaline slag is taken, sodium peroxide 5g, ore grinding 10min is added, guarantees that -200 mesh account for
82%, 250mL water is added, 100r/min high-speed stirred, 80 DEG C of extraction temperature, extraction time 60min, filtering gained filtrate is
The mixed solution of containing sodium carbonate and natrium arsenicum, leached mud return to antimony smelting system.Secondly it is 1% carbon that concentration is added into electrolytic cell
Acid sodium solution is electrolysed with ferroelectricity extremely anode using carbon resistance rod as cathode, and temperature is 50 DEG C, current density 25mA/
cm2, time 35min, in anode region generation active Fe2+Leaching liquor of arsenic-containing alkaline dregs in electrolytic cell, electricity is added by constant flow pump in ion
Current density is about 20mA/cm2, electrolysis time 1h.With the process of reaction, oxygen evolution in system, ferrous hydroxide poly
Body is oxidized to ferric hydroxide colloid, and arsenate ionic adsorption is on iron hydroxide surface and generates ferric arsenate, is separated by filtration, gained slag
It is changed into As through pyrogenic attack2O5Or simple substance As carries out curing process, filtrate is sodium carbonate liquor, is returned after crystallized processing
Antimony smelting system.Arsenic alkaline slag and sodium carbonate product composition are analyzed as follows table 1.Antimony content is 0.11% in sodium carbonate product, and arsenic contains
Amount is 0.91%, illustrates that the separating effect of arsenic and antimony and alkali is obvious.
1 arsenic alkaline slag of table and sodium carbonate product analysis
Embodiment 2
The secondary arsenic alkaline slag in Hunan antimony smeltery is handled using this process, waste acid As content is up to 10.28%, Sb and contains
Amount 4.12%, carbonate content 26.61%.50g arsenic alkaline slag is taken, sodium peroxide 12g, ore grinding 10min is added, guarantees that -200 mesh account for
86%, 250mL water is added, 80r/min high-speed stirred, 85 DEG C of extraction temperature, extraction time 60min, filtering gained filtrate is
The mixed solution of containing sodium carbonate, natrium arsenicum, leached mud return to antimony smelting system.Secondly it is 1% carbon that concentration is added into electrolytic cell
Acid sodium solution is electrolysed with ferroelectricity extremely anode using carbon resistance rod as cathode, and temperature is 60 DEG C, current density 30mA/
cm2, time 30min, in anode region generation active Fe2+Leaching liquor of arsenic-containing alkaline dregs in electrolytic cell is added by constant flow pump in ion,
Current density is about 20mA/cm2, electrolysis time 1.5h.With the process of reaction, oxygen evolution in system, ferrous hydroxide
Polymer is oxidized to ferric hydroxide colloid, and arsenate ionic adsorption is on iron hydroxide surface and generates ferric arsenate, is separated by filtration, institute
It obtains slag and is changed into As through pyrogenic attack2O5Or simple substance As carries out curing process, filtrate is sodium carbonate liquor, after crystallized processing
Return to antimony smelting system.Arsenic alkaline slag and sodium carbonate product composition are analyzed as follows table 2.Antimony content is 0.15% in sodium carbonate product,
Arsenic content is 0.22%, illustrates that the separating effect of arsenic and antimony and alkali is obvious.
2 arsenic alkaline slag of table and sodium carbonate product analysis
Claims (6)
1. the electrochemical method of arsenic and alkali in a kind of separation arsenic alkaline slag, it is characterised in that: the following steps are included:
1) arsenic alkaline slag is subjected to oxidation water logging, obtains the leaching liquor of arsenic-containing alkaline dregs of containing sodium carbonate and natrium arsenicum；
2) it is cathode by electrolyte, ferroelectricity extremely anode and carbon electrode of sodium carbonate liquor, is electrolysed, is generated in the electrolytic solution
Active ferrous hydroxide；The mass percent concentration of sodium carbonate is 0.5~1% in electrolyte, and electrolyte temperature is 50~60 DEG C,
Current density is 20~40mA/cm2, electrolysis time is 20~40min；
3) 1) gained leaching liquor of arsenic-containing alkaline dregs in is added into the electrolyte containing active ferrous hydroxide in 2), is electrolysed, it is raw
At ferric arsenate crystal settling.
2. a kind of electrochemical method for separating arsenic and alkali in arsenic alkaline slag according to claim 1, it is characterised in that: by arsenic alkaline slag
By ore grinding and water logging is added to go out with oxidant, is separated by solid-liquid separation, obtains the leaching liquor of arsenic-containing alkaline dregs of containing sodium carbonate and natrium arsenicum.
3. a kind of electrochemical method for separating arsenic and alkali in arsenic alkaline slag according to claim 2, it is characterised in that: the arsenic alkali
Slag and oxidant ore grinding to granularity meet -200 mesh granular mass degrees and account for 80% or more.
4. a kind of electrochemical method for separating arsenic and alkali in arsenic alkaline slag according to claim 3, it is characterised in that: the oxidation
Agent is sodium peroxide, the relative usage of the oxidant be arsenite in arsenic alkaline slag and antimonite are oxidized to arsenate and
1~1.2 times of oxidant theoretical molar amount needed for stibate.
5. a kind of electrochemical method for separating arsenic and alkali in arsenic alkaline slag according to claim 2, it is characterised in that: the oxidation
Leaching condition are as follows: liquid-solid ratio L/S is 3~6mL/1g, and stirring rate is 80~100r/min, and extraction temperature is 80~85 DEG C, leaching
0.5~1.5h of time out.
6. a kind of any one electrochemical method for separating arsenic and alkali in arsenic alkaline slag, feature exist according to claim 1~5
In: 3) electrolytic condition in are as follows: electrolyte temperature is 50~60 DEG C, and current density is 10~30mA/cm2, electrolysis time 1h
~1.5h.
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